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Part A: Precipitation hardening in a TI-CU alloy Part B: The structural and nagnetic Properties of… Howe, Lawrence Martin 1956

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PART A:  PRECIPITATION HARDENING IN A TI-CU ALLOY  PART BJ  THE STRUCTURAL AND MAGNETIC PROPERTIES  OF SOME QUARTERNARY ALLOYS OF Mn^oAlZn o^ C20 x  2  x  AND Mn^Ga^Zngo^CgQ  by  LAWRENCE MARTIN HOWE  A THESIS SUBMITTED IN PARTIAL FULFILMENT OF THE REQUIREMENTS FOR THE DEGREE OF MASTER OF APPLIED SCIENCE  i n the Department of MINING.AND METALLURGY We accept t h i s thesis as conforming t o the standard required from candidates f o r the degree of MASTER OF APPLIED SCIENCE.  Members of the Department o f Mining and Metallurgy.  THE UNIVERSITY OF BRITISH COLUMBIA August,  1956  ABSTRACT  The decreasing s o l i d s o l u b i l i t y l i m i t at the titaniumr i c h end of the titanium-copper c o n s t i t u t i o n a l diagram suggests the p o s s i b i l i t y that titanium-rich alloys may be age-hardenable.  However,  r e s u l t s obtained by previous investigators, using lump samples, show that a f t e r quenching from 790°C the age-hardening of an a l l o y containing 1,7 percent copper i s very light while a 0.8 percent copper a l l o y decreases i n hardness, during heat treatment at 400°C, It was believed possible that powder samples of alloys might show d i f f e r e n t r e s u l t s from the lump samples used by previous investigators.  Consequently, a 1.90 percent copper a l l o y was made by  the technique of l e v i t a t i o n melting, checked f o r homogeneity, and f i l i n g s of 48-65 Tyler screen size were cut from i t f o r aging experiments. Hardness readings do show a hardness peak at aging temperatures of 400°C, 450°C, and 500°C and thus indicate that the titanium-copper a l l o y i s susceptible to age-hardening treatments. Interest i n the Mn oAl Zn2o_ '20 (  D  x  x  a n d  ^ 6 0 x 2 0 - x C 2 0 y tems Ga  Zn  s  8  r e s u l t s from pregious studies of Mn-Al-C, Mn-Zn-C, and Mn-Ga-C systems; i n p a r t i c u l a r the alloys near compositions ^n^^A^o^o* M^O^^O^O' Mn  an(  *  60Ga 0 20» c  2  The saturation magnetization (cr) versus temperature curve f o r a l l o y s near the compositions MnkQA^QC^o  a n c  (T)  * Mn6oG 20^20 h°ws a  s  normal ferromagnetic behaviour from 0°K to the Curie points of the a l l o y s . Alloys near the composition Mn5oZn2oC20>  o  n  t n e  other hand, have abnormal  behaviour as they experience a maximum i n thecr-T curve i n the of -40°C.  neighbourhood  Reasons f o r i n v e s t i g a t i n g the Mn6o^-^ 20-x^20 n  6111(1  ^ 60^ x^ 20-x^20 systems were: n  a  n  1. to provide further data regarding the presence o f abnormal behaviour i n Mn^QZ^o^O Mn6oGa2QC2o»  a  n  d  °^  n  o  r  m  a  l  behaviour i n  Mn^QALgo^o and  ( i . e . a l l o y s near these compositions).  2. to suggest how the valency of the cube-corner atom affects the normal ferromagnetic moment of these a l l o y s . However, investigation of these systems has lead to even more complicated phenomena, and the above two items remain, t o a large extent, unsolved.  ACKNOWLEDGEMENT  The author i s g r a t e f u l f o r f i n a n c i a l a i d i n the form of a research assistanceship provided by the Defence Research Board of Canada. The p r e c i p i t a t i o n hardening studies i n the Ti-Cu a l l o y were o r i g i n a l l y started by E. Saaremaa i n p a r t i a l f u l f i l m e n t of B.A.Sc, requirements.  This work i s part of a program sponsored by the Defence  Research Board of Canada, Project Number 7501-18. Funds f o r the magnetic studies were provided by the Defence Research Board under Research Grant 281. Assays were required f o r the Mn oAl Zn2o_ C2o 0  x  x  a n (  * ^ 6oOa Zn2o_ ^20 n  x  x  a l l o y s and these were k i n d l y done by the Cosma Testing Laboratories i n Cleveland, Ohio. The author i s g r a t e f u l f o r the assistance of the s t a f f of the Department of Mining and Metallurgy.  S p e c i a l thanks are extended to  Dr. J . Gordon Parr, d i r e c t o r of the Ti-Cu research, Dr. H.P. Myers, director of the magnetic research, and R.G. Butters f o r t e c h n i c a l advice and encouragement.  TABLE OF.CONTENTS PART A:  PRECIPITATION - HARDENING IN A TI-CU ALLOY  I.  INTRODUCTION  II.  PREVIOUS WORK  Page .  1 3  I I I . EXPERIMENTAL PROCEDURE 1. Preparation of the alloys  4  2. Heat treatments  5  3. Microhardness measurements  5  IV.  RESULTS  7  V.  DISCUSSION OF RESULTS AND CONCLUSIONS  9  VI.  BIBLIOGRAPHY  PART B:  . . . . .  10  THE STRUCTURAL AND MAGNETIC PROPERTIES OF SOME QUATERNARY ALLOYS OF Mn6oAlxZn20-x 20 C  I.  INTRODUCTION  II.  PREVIOUS WORK  a  n  d  Mn  60 x 20-x°20 Ga  Zn  11  1. Mn-Al-C system  14  2. Mn-Zn-C system . .  15  3. Mn-Ga-C system  16  I I I . EXPERIMENTAL PROCEDURE  IV.  1. Preparation of a l l o y s  19  2. Magnetic measurements  19  3. X-ray measurements and mircroscopic examination  20  RESULTS 1. Mn6oAl Zn20-xC20 system  22  2. Mn6oGa Zn20-x 20 system  32  x  c  x  V.  DISCUSSION OF RESULTS AND CONCLUSIONS . .  37  VI.  BIBLIOGRAPHY  42  ILLUSTRATIONS PART A : 1.  a  Page s o l i d s o l u b i l i t y and e u t e c t o i d r e g i o n on t h e h i g h  t i t a n i u m s i d e of t h e T i - C u phase diagram ( a f t e r  Joukainen  2  et a l ) 2.  E f f e c t o f 400°C a g i n g on hardness o f T i - C u a l l o y s  (both  i n lump form) s o l u t i o n a n n e a l e d i n t h e a f i e l d as determined by Holden e t a l  3  3.  Photograph o f a l e v i t a t i o n - m e l t i n g u n i t i n o p e r a t i o n  4*  Photograph o f a t y p i c a l t i t a n i u m a l l o y i g n o t  5.  E f f e c t o f 4CO°C, 4 5 0 ° C , 500°C a g i n g on hardness of a  . . .  6 •  6  1.90$ Cu a l l o y , i n powder f o r m , as d e t e r m i n e d by t h e a u t h o r  8  PART B : 1,  G e n e r a l r e l a t i o n between s a t u r a t i o n v a l u e and t e m p e r a t u r e  f o r ferromagnetics 2,  2  31101  ^O^ZO ^ 0  1 3  S a t u r a t i o n m a g n e t i z a t i o n versus temperature f o r a l l o y s n e a r t h e c o m p o s i t i o n s Mn£,oAl2oC20»  4.  Mn  60 20 20* Ga  c  V a r i a t i o n of s a t u r a t i o n magnetization w i t h  M n  60 20 20 Z n  C  x  2  x  25  V a r i a t i o n of s a t u r a t i o n m a g n e t i z a t i o n w i t h temperature f o r h i g h aluminum content a l l o y s i n t h e Mn6oAlxZn20-x^20 system  6,  ^  temperature  f o r h i g h z i n c c o n t e n t a l l o y s i n the Mn5QAl Zn o_ ^20 system 5.  11  The p e r o v s k i t e s t r u c t u r e f o r Mn6c-Al2Q.C20>  Mn6oGa QC20» 3.  .......  26  V a r i a t i o n o f s a t u r a t i o n m a g n e t i z a t i o n a t 0°K w i t h a t o m i c p e r cent aluminum f o r the Mn^oAl Zn o- C20 x  2  x  system  27  ILLUSTRATIONS (continued) 7«  Page  Bohr magneton value versus atomic percent aluminum for the Mn6oAl Zn20-x^20 system  . . . . .  x  8.  Variation of Curie temperature with atomic percent aluminum i n the Mn5QAl Zn2o_ ^20 system x  9,  29  x  Variation of lattice parameter with atomic percent aluminum for the Mn QAl Zn20-x 20 system  30  c  x  o  10.  Comparison of X-ray intensity plots at -186°C and 20°C for a 2.85$ Al alloy  11.  31  Variation of saturation magnetization with temperature for alloys in the Mn5oGa Zn20- ^20 system . o . . . . . . . x  12.  x  M  Ga  Zn  s  ^4  s t e m  0  Bohr magneton value versus atomic percent gallium for the Mn£, Ga Zn2o_ C o system 0  14.  x  x  35  2  Variation of lattice parameter with atomic percent gallium for the ^6o x 20-x^20 system Ga  15.  33  Variation of saturation magnetization with atomic percent gallium for alloys i n the n o x 2 0 - x ^ 2 0 y  13.  28  36  Zn  Variation of Bohr magneton value with lattice parameter  for M n A l C 2 , ^ H c ^ o C g o , and Mn^oZr^^o 60  20  0  ,  39  PART A:  PRECIPITATION HARDENING IN A TI-CU ALLOY  I.  INTRODUCTION  The necessary condition f o r carrying out a p r e c i p i t a t i o n hardening process on an a l l o y i s that at room temperature there s h a l l be present i n the slowly cooled a l l o y a large amount of one phase and a smaller amount of a second phase. of the  The f i r s t constituent must be capable  dissolving a l l or an appreciable amount of the second constituent as temperature i s r a i s e d . The decreasing s o l i d s o l u b i l i t y l i m i t at the titanium-rich  end of the titanium-copper c o n s t i t u t i o n a l diagram"*" (Figure l ) suggests the  p o s s i b i l i t y that titanium-rich alloys may be age-hardenable.  Re-  f e r r i n g to Figure 1, we see that at 79&°C, copper i s soluble i n titanium to 0.5  the extent of 2 , 1  percent, whereas the s o l u b i l i t y i s approximately  percent at room temperature. Ordinarily, concentrations of the hardening constituent  approaching maximum s o l i d s o l u b i l i t y i n the a phase at the eutectoid temperature are chosen. the  The f i r s t step i n the heat treatment i s to heat  a l l o y to a temperature i n the a phase f i e l d i n order to obtain a  s o l i d s o l u t i o n of uniform composition.  The saturated solution thus  formed i s quenched or at l e a s t cooled at too rapid a rate to permit the separation of the second phase that would normally occur with slow cooling. As a r e s u l t of the r a p i d cooling, the a l l o y i s i n a state of supsrsaturation and i s therefore thermodynamically unstable. The subsequent age-hardening of the a l l o y i s a r e s u l t of the decomposition of the solution, which i n some a l l o y s occurs at ordinary room temperatures but usually requires a r e l a t i v e l y low temperature heat treatment.  - 2 -  500 l.<J©% 2  3  4  5  6  7  8  Weight Percent Copper Fifrure 1  a s o l i d s o l u b i l i t y and cutectoid region on the high titanium side of the Ti-Cu phase diagram.  10  - 3 I I PREVIOUS WORK  2 Results obtained by Holden et a l reproduced i n Figure 2 show that a f t e r quenching from 790°C the age-hardening of an a l l o y containing 1.7  percent copper i s very s l i g h t , while a 0.8 percent  a l l o y decreases i n hardness, during heat treatment at 400°C. However Holden et a l used lump samples and i t was believed possible that powder samples of a l l o y s might show d i f f e r e n t results from the lump samples.  Reason f o r believing thusly i s that small  p a r t i c l e s are often more sensitive to d i f f u s i o n processes than larger samples.  150  Aging time i n Hours Figure 2  E f f e c t of 400°C aging on hardness of Ti-Cu alloys solution annealed i n the a f i e l d as determined by Holden, Watts, Ogden, and Jaffee.  - 4 -  III.  EXPERIMENTAL PROCEDURE  Preparation of the A l l o y s . Owing to the high melting-point of titanium (1800°C) d i f f i c u l t i e s are encountered i n melting techniques.  Method adapted was that  3 of melting the titanium a l l o y by l e v i t a t i o n  i n a high-frequency  field.  I n i t i a l preparation involved placing the required amount of copper (1.90 percent by weight) i n a hole d r i l l e d iodide titanium sample.  in a cylindrical  Weight of the prepared specimen was  approximately  6 grams. The titanium-copper  specimen was melted i n about 30  seconds  - and i t remained l e v i t a t e d , without dripping, i n the molten state i n an argon atmosphere (Figure 3).  When the c o i l current i s switched o f f  the metal drops into a copper mold d i r e c t l y below the c o i l .  A typical  ingot i s shown i n Figure 4. ... There was no trace of reaction or s i n t e r i n g between the mold and the a l l o y .  The ingots were shown to be homogenows both by micros -  scopic examination and by the i d e n t i c a l X-ray d i f f r a c t i o n patterns which were obtained from s i m i l a r l y treated samples of d i f f e r e n t parts of the same ingot. Previous investigators i n the department had done checks on contamination.  A piece of pure iodide titanium was melted, cast,  and hardness readings were taken. center to 90 at the outside,  The readings varied from R  F  80 at the  (usual hardness value quoted f o r pure as-  cast titanium i s 70 to 75 Rp )•  The ingot was melted a second and a t h i r d  time and there was no change i n these hardness values.  Therefore, according  to accepted standards, there was no contamination during melting.  - 5 -  •  Heat Treatments. A gas-quenching furnace was used f o r quenching operations. F i l i n g s of 48-65 Tyler screen size were cut from the ingot and placed i n a small molybdenum boat.  The boat and the sample were than placed i n a  furnace, held i n an atmosphere of argon while heated to 790°C f o r several minutes, and then blown out of the heating zone into a f l a s k by a j e t of helium gas. the  No reaction occurred between the f i l i n g s and the boat and  f i l i n g s did not appear to be sintered. For  aging, the f i l i n g s were sealed i n vacuo i n s i l i c a tubes  and aged at temperatures of 400°C, 450 C, and 500°C f o r various time 9  intervals. Microhardness Measurements. Hardness readings were taken on a Bergsman Microhardness Tester, using a 25 gram load applied to a diamond indenter. F i l i n g s were mounted i n l u c i t e f o r this t e s t .  Figure 4  Photograph of t y p i c a l titanium a l l o y ingot.  - 7 -  IV.  RESULTS  Hardness readings taken at various time i n t e r v a l s f o r aging temperatures of 400°C, 450°C, and 500°C are plotted i n Figure 5.  From  t h i s graph i t i s seen that a hardness peak i s obtained at each aging temperature. About a dozen readings were taken on each heat-treatment sample; the highest reading and the lowest reading were ignored and an average taken of the remaining values.  In Figure 5 the curves pass  through the average readings while the extent of scatter i s shown by the length of the v e r t i c a l l i n e s drawn through each point on the curves. Micro-structures of a l l samples were examined and X-ray goniometer plots were taken between 20 values of 34° and 44° f o r as quenched, age-hardened  10 minutes, and age-hardened 1000 minutes samples f o r a l l  three aging temperatures.  Microstructures showed the presence of a only  and likewise Xrray goniometer plots only revealed the presence of closepacked hexagonal a l i n e s namely: 40.1°.  100 at 35°, 002 at 38.2°, and 101 at  No l i n e s at 39*5° and 43° c h a r a c t e r i s t i c of T i Cu were present,  (above angles are 26 values).  2  Aging Time i n Minutes Figure 5  E f f e c t of 400°C, 450°C, 500°C aging on hardness of 1.90$Cu a l l o y , i n powder form, as determined by author.  - 9  V.  -  DISCUSSION OF RESULTS AND CONCLUSIONS  Microscopic and X-ray examinations failed to reveal any structural changes during the aging process.  This is not too surprising  since early stages of precipitation do not usually manifest themselves in ways that are readily detectable by metallographic methods and the extent of precipitation on overaging a 1.90 percent copper alloy is very small. It i s generally accepted that during aging some hardening occurs as a result of stresses set up by 'pre-precipitation* processes. At low temperatures of aging actual precipitation never occurs and hence the hardness curve i s asymptotic to a line parallel to the time axis.  At  higher temperatures of aging precipitation occurs, stresses are relieved, and the hardness curves f a l l off. In the titanium-copper alloy at temperatures between 400°C and 500°C the hardness curves show characteristics that are typical of overaging.  Experiments conducted at lower temperatures by other investi-  gators, also using powdered samples, gave no positive indication of hardness increase. Therefore, i t appears that the coherency between the precipitate and the matrix material is short lived at the temperatures investigated - a fact which may be peculiar to the titanium-copper system or to the use of samples of very small dimensions. Quite apart from this 'overaging* preculiarity, the results indicate that the titanium-copper specimens are readily susceptible to age hardening treatments.  +  This is i n contrast with the behaviour of lump  samples which are reported by other workers  2  to respond negligibly.  - 10 VI.  BIBLIOGRAPHY  1.  A Joukainen, N.J. Grant, C F . Floe, Trans A.I.M.E. (1952), 194, 766.  2.  F.C. Holden, A.A. Watts, H.R. Ogden, R.I. Jaffee, Trans A.I.M.E.  (1955), 203, 117. 3.  D.H. Polonis, R.G. Butters, J.G. Parr, Research (1954), 7, 10s.  4.  D.H. Polonis, J.G. Parr, Trans A.I.M.E. (1954), 200, 1148.  - 11 PART B:  THE STRUCTURAL AND MAGNETIC PROPERTIES OF SOME  QUATERNARY ALLOYS OF Mn6oAl Zn o_x 20 G  x  I.  ANI1  2  Mn  60 x 20-xC20 Ga  Zn  INTRODUCTION  Weiss , i n his molecular f i e l d approach to magnetism, obtains 1  the f o l l o w i n g r e l a t i o n s h i p f o r ferromagnetics: <S/CG= tanh C«se/fl- T) 0  Where o©  a  i s the saturation magnetization at temperature i n question,  i s the saturation magnetization at absolute zero, T i s the temperature,  and 0 i s the Curie point defined by:  Where JX i s the atomic or molecular magnetic moment, K i s Boltzmann's universal gas constant, and N i s the Weiss intermolecular f i e l d  constant.  In the above, Weiss i s using the assumption of quantum theory namely that there are only two directions permissible f o r the spins of the elections i e :  p a r a l l e l and a n t i p a r a l l e l .  The general r e l a t i o n s h i p between saturation magnetization and  1.0 I  0 0 Figure 1  General r e l a t i o n between saturation value and temperature f o r ferromagnetics.  - 12 temperature which i s l i s t e d above i s p l o t t e d i n F i g u r e  1.  The e x p e r i m e n t a l l y observed s a t u r a t i o n v a l u e o f the f e r r o magnetics does i n f a c t  f a l l w i t h r i s i n g temperature r e a c h i n g  substanitally  zero at a temperature known as t h e C u r i e temperature o r magnetic point.  The observed r e l a t i o n s f o r t h e elements i r o n ,  a r e i n good agreement w i t h t h e above A plot o f s a t u r a t i o n value  and n i c k e l  theory. (<Jl) v e r s u s temperature  Hn QAl2QC2Q  a l l o y s near t h e compositions  cobalt,  a  n  (T) f o r  ^ 60 20^20 i n d i c a t e t h a t  d  n  D  Ga  t h e s e a l l o y s obey normal f e r r o m a g n e t i c b e h a v i o u r from a b s o l u t e t o the C u r i e p o i n t s . do n o t e x h i b i t  change  However, a l l o y s near t h e c o m p o s i t i o n  zero  Mn QZn2oC20 D  normal f e r r o m a g n e t i c behaviour as a maximum o c c u r s i n t h e  C" - T curve a t a p p r o x i m a t e l y -40°C. In o r d e r t o o b t a i n f u r t h e r i n f o r m a t i o n w i t h r e g a r d t o t h i s abnormal behaviour , i t was desirfjable  to investigate  p e r t i e s o f t h e systems Mn oAl Zn Q_ C2o x  0  2  a  t h e magnetic  pro-  d M^oG^xZr^O-xC^O*  n  x  A l l o y s o f t h e c o m p o s i t i o n s Mn QAl oC2o> 0  2  M 6oO 20^20 n  a  a  n  d  ^602^20^20 have a h i g h l y - o r d e r e d s t r u c t u r e i n which manganese o c c u p i e s face-center  p o s i t i o n s of cube,  carbon o c c u p i e s t h e b o d y - c e n t e r  and aluminum, g a l l i u m , o r z i n c atoms are a t the cube c o r n e r s . s t r u c t u r e appears i n F i g u r e  The proposed  2.  Through an i n v e s t i g a t i o n o f systems,  position,  i t was thus a l s o d e s i r e d t h a t  Mn oAl Zn2o_ C2o 0  x  x  a  n  d  Mn  60 x 20-x '20  alloys.  Zn  <  i n f o r m a t i o n c o u M be o b t a i n e d which  would suggest how the v a l e n c y o f t h e c u b e - c o r n e r atom a f f e c t s f e r r o m a g n e t i c moment o f t h e s e  Ga  t h e normal  - 13 -  Figure 2  The proposed structure of Mn Al2oC20> 60 20 20» Mn60Zn20C20« o0  M n  G a  c  a  n  d  - 14 -  II.  PREVIOUS WORK  Mn-Al-C System  2 Butters and Myers ^ 6oAl20 20 n  G  >  investigated a l l o y s close to the composition  For a f i x e d carbon content of 20 atomic percent the single  face-centered cubic structure occurs over the composition range Mn 60-69 atomic percent (hence A l 2 0 - 1 1 atomic percent). Increasing the manganese content beyond 60 atomic percent to 70 atomic percent causes an increase i n the Curie temperature  from 0°C to  300°C, a decrease i n the saturation magnetization from 1 . 2 0 to approximately 0.6 Bohr magnetons per manganese atom, and a s l i g h t increase i n the l a t t i c e paramater from 3.869A to 3.874A . 0  0  This decrease i n magnetization as the  manganese content i s increased past 60 atomic percent can be explained by assuming that the magnetization of the a d d i t i o n a l manganese atoms, which must replace aluminum atoms i n cube corner positions, i s a n t i p a r a l l e l to that of those i n the face-centered positions.  The magnitude of the  decrease i n magnetization corresponds to the extra manganese atoms having an e f f e c t i v e Bohr magneton value of -4. In these alloys the saturation magnetization below the Curie temperature varies with temperature  i n a normal ferromagnetic manner as  can be seen i n Figure 3 f o r an a l l o y near the composition Mn oAl2oC20* 0  Paramagnetic behaviour above the Curie point seems to indicate ferrimagnetisra, however neutron d i f f r a c t i o n results indicate that Mn6oAl2oQ20^magnetic.  s  ferro-  - 15 -  Mn-Zn-C System Butters and Myers-' also investigated the behaviour of alloys near the composition Mn^QZ^gC^O'  w  i  t  n  i  n  t n e  range of composition studied,  C 20 atomic percent, Zn 10-20 atomic percent, Mn 70-60 atomic percent, i t was found that the structure of the alloys was face-centered cubic.  In-  creasing the manganese content beyond 60 atomic percent to 70 atomic percent causes an increase i n the Curie point from 80° to 488°C and a decrease of the l a t t i c e parameter from 3.925A° to 3.899A . 0  For a l l o y s with a zinc content above 15 atomic percent a marked maximum i n the magnetization occurs i n the, region of -40°C to -50°C.  Above  t h i s temperature the magnetization decreases i n the usual fashion becoming zero at the Curie point.  Below t h i s temperature region the magnetization  decreases but the decrease becomes less the lower the temperature. abnormal behaviour f o r an a l l o y near composition Mn QZn2oC2o ^ Q  Figure 3 .  s  This  shown i n  Also, for t h i s a l l o y , i t was found that at -186°C the o r i g i n a l  face-centered cubic structure observed at room temperatures i s s l i g h t l y distorted becoming face-centered tetragonal with a=3.921A° and c/a=0.9947. Neel has shown that the magnetization of a ferrimagnetic substance may vary with temperature i n a s i m i l a r manner to the abnormal be^ haviour observed i n above Mn-Zn^-C a l l o y s .  Paramagnetic behaviour above  the Curie point also appears to agree with that predicted by Neel f o r ferrimagnetics. However, results obtained by Dr. B. Brockhouse at Chalk River, using neutron d i f f r a c t i o n techniques, seem to suggest a different magnetic concept.  The concept proposed i s that of opposing sublattices having  different Curie points (the sublattices of a ferrimagnetic substance have the same Curie points).  - 16 -  The Curie point of one sublattice i s assumed to be -40°C, where the maximum i n the saturation magnetization of Mn QZn2oC20 occurs. 0  The other Curie point i s at 100°C as observed by magnetic measurements. The resultant magnetization i s a vector sum of the opposing sublattices. It i s also rather interesting to note that a second order s p e c i f i c heat anomaly corresponding to the Curie point of one sublatticeshould occur at -40°C. ments on Mn^QGa2QC2o ^  Such an anomaly has been found to exist i n measurey  M. Swanson, here at the department.  Mn-Ga-C System Butters and Myers started t h i s study and the project was then continued by the author.  X-ray Debeye-Bcherrer d i f f r a c t i o n photographs  show that, within range of composition, C 20 atomic percent, Mn 62-70 atomic percent, Ga 10-18 atomic percent, the a l l o y s have a face-centered cubic structure. Mn£,oGa2oC20  a  s  It was not possible to obtain an a l l o y of composition  made up alloys of t h i s composition contained free carbon.  Saturation magnetization v a r i a t i o n with temperature  f o r alloys  indicated normal ferromagnetic behaviour such as that i l l u s t r a t e d i n Figure 3 f o r an 18 atomic percent gallium a l l o y .  The l a t t i c e parameter increases  with increasing manganese content from 3.876A at 62 atomic percent manganes 0  to 3.881A , whereas the Bohr magneton value per manganese atom decreases 0  from a value of 1.27 at 62 atomic percent manganese to 0.62 at 70 atomic percent manganese. This would seem to suggest that the additional manganese atoms (in excess of 60 atomic percent) are replacing the gallium atoms at the cube corners and the magnetization of the cube corner manganese atoms  - 17 -  i s a n t i p a r a l l e l to that of those i n face-centered positions.  The magnitude  of the decrease corresponds to a value of - 4 Bohr magnetons f o r the extra manganese atoms„  - 18 -  100  200  300  400  Temperature °K Figure 3  Saturation magnetization versus temperature f o r alloys near the compositions Mn oAl2()C20» ^ 60 J 20p20> and Mn6oZn2oC20• n  D  (  a  - 19 -  III.  EXPERIMENTAL PROCEDURE  Preparation of Alloys The materials used i n the preparation of the a l l o y s f o r t h i s work were manganese of 9 9 . 9  of 99.99 percent purity,  percent p u r i t y , zinc  aluminum of 99.99 percent p u r i t y , gallium of 99.99 percent purity and graphite of spectroscopic grade  0  The f i r s t step i n the preparation of the alloys was Mn-Al-C and Mn-Ga-C master a l l o y s .  Melting was  to make  carried out by the process  of induction heating under an atomosphere of argon a f t e r i n i t i a l evacuation and degassing.  Melts were c h i l l cast under argon into a s p l i t brass mold.  Ingots were annealed i n vacua i n quartz tubes to remove coring and promote homogeneity.  Zinc  could not be included i n t h i s melting stage due to  i t s low d i s t i l l a t i o n  temperature.  Master alloys were then crushed and mixed with the appropriate amount of zinc of powders was  f i l i n g s to produce the mixture f o r s i n t e r i n g .  The mixture  placed i n a clean fused quartz tube, the tube was  and sealed, and the s i n t e r i n g was mately one week.  evacuated  achieved by heating to 600°C for approxi-  In some cases the a l l o y s were recrushed and resintered.  The sinters wer homogeneous but tended to decompose i f l e f t i n moist a i r f o r long periods.  They were therefore kept i n a dessicator  when not i n use. Magnetic Measurements For the magnetic measurements- an external f i e l d of 16,200 oersteds was used.  The f i e l d was  obtained by means of an electromagnet having i t s  poles shaped so that a uniform f i e l d gradient was considerably greater than that of the specimen.  produced over a volume  - 20 -  A Sucksmith r i n g balance was used to measure the magnetization. The p r i n c i p a l involves the comparison of the forces exerted i n turn on a sample of a l l o y and a sample of i r o n under i d e n t i c a l conditions.  The  magnetic properties of pure iron being accurately known, those of the a l l o y sample may be calculated. The a l l o y specimen  experiences a force F  x  given by:  whereCis the saturation magnetization,m i s the mass, and &\\/A-x i s the f i e l d gradient. Under i d e n t i c a l conditions an i r o n standard experiences a force: F. = 0- rt\, <JH/<ix s  The forces F  x  and F  s  are balanced by the restoring force of a  beryllium copper ring and the displacement of the specimen i s measured by a displaced l i g h t beam passing through two mirrors attached to the r i n g . We thus obtain: K<J»= F = 6-*n>xoH/dx x  from which:  About 30-40 mg. of sintered a l l o y was used f o r measurement, t h i s being placed i n a platinum-iridium container.  A furnace and dewar  attachments permitted measurements over temperature range required namely between -190°C and Curie points (highest about 230°C). Paramagnetic measurements were not made as there would have been trouble a r i s i n g due to the d i s t i l l i n g out of zinc at elevated temperatures. X-ray Measurements and Microscopic Examination Debeye-Sherrer powder photographs were taken and the l a t t i c e paramaters were calculated from these i n the usual way.  Low temperature  X^ray i n t e n s i t y plots were made on alloys of high zinc content i n  -  21 -  Mn^QAl Zn2o_ C20 system using a Geiger counter spectrometer. x  x  Samples were mounted i n l u c i t e , polished, etched with 4 percent n i t o l solution, and observed under the microscope.  This examination  served as an a d d i t i o n a l check as to whether the a l l o y s were single phase or not.  - 22 IV. RESULTS  MnAnAlyZn?o.vC2o System In Figures 4 and 5 the v a r i a t i o n of saturation magnetization (o~) with temperature  (^) j _ shown f o r single phase a l l o y s . s  Normal  ferromagnetic behaviour i s experienced by single phase alloys of aluminum content of approximately 5.5 atomic percent and up.  Alloys with lower  aluminum contents than 5.5 atomic percent have a maximum or very f l a t portion i n t h e i r saturation magnetization curves. of  An a l l o y consisting  9.6 atomic percent aluminum was also studied and was found to have  normal ferromagnetic behaviour but i s not included on the graphs f o r sake of  clarity. The point at which deviation from normal ferromagnetic be-  haviour occurs s h a l l be referred to as the t r a n s i t i o n point, t r a n s i t i o n temperature  or simply t r a n s i t i o n .  The t r a n s i t i o n temperatures f o r 0,  2.85,  and 4.6 atomic percent aluminum alloys are 231-2, 210±5, and 120±10°K respectively. In Figure 6 the saturation magnetization at 0°K (cs)  i s plotted  against atomic percent aluminum.  Normal ferromagnetic a l l o y s are repre-  sented by only one point namely  -ordinary which was obtained by an extra-  polation of the 0*-T  curve.  Alloys which do not have normal ferromagnetic  behaviour are represented by two points namely 61 -ordinary and ordinary.  fii-extra-  The f i r s t of these represents an extrapolation of the tf"-Tcurve  (to absolute zero) above the t r a n s i t i o n temperature  i . e . region c h a r a c t e r i s t i c  of a normal ferromagnetic. C7 extra-orindary represents an extrapolation 0  of the CT-T curve below the t r a n s i t i o n temperature.  V e r t i c a l and horizontal  - 23 -  l i n e s through the points represent the deviations to be expected i n the <r-T  extrapolations and i n the aluminum compositions.  Single phase a l l o y s  were not obtainable between 10 and 16 atomic percent aluminum and the dotted l i n e represent form of curve expected i f they were obtainable. The Bohr magneton values have been calculated and then plotted versus atomic percent aluminum.  Even though deviations are not shown  i t i s to be understood that they are s t i l l applicable.  Curve i s shown  i n Figure 7. Curie temperatures were obtained from cr* versus T curves and are plotted versus aluminum content i n Figure 8.  The v a r i a t i o n of Curie  temperature with composition c e r t a i n l y i s of a rather complex form and since probably very l i t t l e i s to be gained from a study of same i t s h a l l not be discussed further. X-ray Debeye-Sherrer powder photographs show l i n e s c h a r a c t e r i s t i c of a face-centered cubic and also superlattice l i n e s .  Lattice parameters  f o r single phase alloys decrease l i n e a r l y from Mn0oZn2oC20 *° ^"60^1-20^20 as can be seen from Figure 9.  Dotted region of curve i s that i n which single  phase alloys were not obtainable. X-ray l i n e i n t e n s i t y plots were obtained at -186°C and 20°C f o r a l l o y s of 2.85, s u l t s f o r a 2.85  5.5, and 7.5 atomic percent aluminum. percent a l l o y are shown i n Figure 10.  Photographs of reFrom an examination  of the photographs i t i s noted that there i s a d e f i n i t e broadening of 220 and 311 l i n e s at -186°C whereas the 111 l i n e remains unchanged.  It appears  that 220 and 311 l i n e s are s p l i t t i n g into two components at -186°C but t h i s i s not too well resolved.  Results f o r the 5.5 and 7.5  percent alloys  are not displayed but i t was found that the i n t e n s i t y plots gave no i n d i cation of s p l i t t i n g or broadening of l i n e s occurring.  -2k-  Let us consider f o r a moment the t r a n s i t i o n from a cubic to a tetragonal structure.  Upon examination of the structures i n question i t  can be seen that as a structure changes from cubic to tetragonal one expects no s p l i t t i n g of X-ray l i n e s f o r 111 and 222 planes. expects s p l i t t i n g of l i n e s f o r 200,  220,  components with m u l t i p l i c i t y factors of  311, 2:1.  On the other hand one  and 400 planes into two  - 25 -  100  90 T3 CD  »  M «>  80  o  70 01  ttO  O  60  c o  •H -P cfl N •H -P  50  (1)  C  a o  •H -P nS f-. -P  al  CO  40  30 20  10  100  200  ' 300  400  Temperature °K Figure 4  Variation of saturation magnetization with temperature f o r high zinc content a l l o y s i n the M n ^ A l Z n system. 2  500  - 26 -  Figure 5  Variation of saturation magnetization with temperature  f o r high aluminum content alloys  i n the M n 6 0 x 2 0 - x 2 0 A 1  Z n  C  s  v  s  t  e  m  '  - 27 -  50  [  _j  | 4  2  j  i 8  6  i 10  i  12  i 14  i 16  Atomic Percent Aluminum  Figure 6  V a r i a t i o n of saturation magnetization at 0°K with atomic percent aluminum f o r the M N  60 x A 1  Z N  20-x 20 C  s  ys m. te  i 18  20  - 28 -  o  0..8  _  0.7  -  0.6  -  0.5  1  I  l  2  4  I  6  ordinary pa  l  I  i  l  I  8  10  12  14  16  i  18  Atomic Percent Aluminum Figure 7/ Bohr magneton value versus atomic percent aluminum f o r the Mh ()Alx 20-x^20 sy ^* ' Zn  D  3  111  - 29 -  Atomic Percent Aluminum Figure 8  Variation of Curie temperature with atomic percent aluminum i n the Mn Al Zn _ C system. 6 0  x  2 0  x  2 0  - 30 -  3.950 _  3  - 50 I 8  l 2  i 4  i 6  i 8  i 10  i 12  • 14  i 16  i 18  20  Atomic Percent Aluminum  Figure 9  The v a r i a t i o n of l a t t i c e parameter with atomic percent aluminum f o r the Mn^QAl^Z^o-x^O system.  - 31 -  Figure 10  Comparison of I-ray i n t e n s i t y plots at -186°C and 20°C f o r a 2.85$ A l a l l o y .  - 32 MnooGa^nao-x^O System The v a r i a t i o n of saturation magnetization with temperature f o r single phase a l l o y s i s shown i n Figure 11 greater than 6.63  8  Alloys with gallium content  atomic percent, which would be expected to show normal  ferromagnetic behaviour, by analogy with Mn6oA^x 20-x^20 system, are Zn  not single phase unfortunately and hence cannot be considered,, with gallium contents less than 6.63  Alloys  atomic percent experience the same  magnetic phenomena as i n the aluminum system. Saturation magnetization versus atomic percent gallium and Bohr magneton values versus atomic percent gallium were plotted and appear i n Figures 12 and 13 respectively. applies as that outlined i n the  The same i n t e r p r e t a t i o n of these graphs  Mn6oAl Zn2o C20 section. x  temperatures f o r a l l o y s o f 0,1.87 , and  Transition  =x  3.79 atomic percent gallium are  231^2, 210±5, 185*5°K respectively. Curie temperatures were obtained from o^vs. T p l o t s . obtained are gallium is  Values  415-5°K f o r 1.87 percent gallium 390i5°K f o r 3.79 percent  380±5°K f o r 6.63 percent gallium. Expected value f o r Mn^QZ^c^o  353-5 °K (no value obtainable f o r Mn6oGa2C)C2o) • ^  n e  v  a  l  u  e  s  were not  plotted as i t i s f e l t that i t would be o f l i t t l e use ..since no simple r e l a t i o n s h i p appears to exist between composition and Curie temperature f o r these a l l o y s just as f o r the a l l o y s i n the aluminum system. Single phase alloys exist only up to gallium concentration o f atomic percent.  6.63  In t h i s region X-ray Debeye-Sherrer powder photographs show  l i n e s c h a r a c t e r i s t i c of a face-centered cubic and also s u p e r l a t t i c e l i n e s . L a t t i c e parameters f o r these single phase a l l o y s are plotted versus gallium content i n Figure 14.  Beyond 6.63  percent gallium another face-centered cubic  phase appears along with the o r i g i n a l face-centered cubic phase.  The f i r s t or  o r i g i n a l phase disappears with even higher gallium contents and i s replaced by a phase o f unknown c r y s t a l structure which coexists with the second facecentered cubic phase.  - 33 -  Figure 11  Variation of saturation magnetization with temperature f o r alloys i n the Mh£ o Zn2o_x '20 system. Ga  )  x  (  -3k-  50 1  I  I  I  I  2  4  6  8  I  10  I  1  1  12  14  16  —I IB  Atomic Percent Gallium' Figure.. 12  V a r i a t i o n of saturation magnetization with atomic percent gallium f o r a l l o y s i n the Mn£j0GaxZn2o_xC2o system.  20  - 35 -  O  Ordinary  0  Extra-ordinary OQ  ^  _L  8  10  12  14  16  18  Atomic Percent Gallium Figure 13  Bohr magneton value versus percent gallium f o r the system.  atomic  6o x^ 20-x^20  Mn  Ga  n  20  - 36 -  Atomic Percent Gallium Figure 14  Variation of lattice parameter with atomic percent gallium for the M L  60 x 20-x 20 G a  Z N  C  S T S T E M  *  - 37 -  V. DISCUSSION OF RESULTS AND CONCLUSIONS  The assay results indicated that i t was rather d i f f i c u l t to obtain a l l o y s , i n theM n 6oAL x Z n 20-x G 20  a n d  lfo  60 x2 20-x^20 systems, Ga  n  by s i n t e r i n g process, which had compositions same as those o r i g i n a l l y desired.  However i n most cases the f i n a l percentages of constituents  were f a i r l y close t o the as-made-up compositions and i n those cases where they were not the a l l o y s were discarded. In order to make p l o t t i n g of graphs and i n t e r p r e t a t i o n of results easier percentages of zinc and aluminum i n Mn^QAl Zn2o_ 20  system were adjusted so that the aluminum plus zinc  G  x  x  atomic percents t o t a l l e d twenty, s i m i l a r l y f o r the gallium and zinc  in  the Mn5oGaxZn2o»xG20 system. ' Manganese and carbon percentages may be considered as being e s s e n t i a l l y 60 and 20 atomic percent respectively as the assay r e s u l t s indicated that i n most cases they were w i t h i n one atomic percent of these f i g u r e s .  V a r i a t i o n t o be expected i n composition  has been shown on graphs or accounted f o r i n some manner and i t i s important to note that even though there i s t h i s s l i g h t v a r i a t i o n i n composition that the general trends as indicated i n the g r a p h s are unquestionably r e l i a b l e . Single phase a l l o y s obtained i n the Mn oAl Zn20-x 20 G  0  ^60 x 20-x^20 Ga  Zn  s  y  s  t  e  m  s  a  n  d  x  were found t o be highly-ordered structures as shown  by Debeye-Sherrer powder photographs and i n f e r r e d from structure determination f o r alloys close to the compositions Mn^QA^e-Cao  a n d Mn  60 20 20'' Zn  c  1 x 1  t h i s  highly-ordered structure manganese occupies face-center positions of cube, carbon occupies the body-center position, and aluminum, gallium or zinc atoms are at the cube corners.  I t i s unfortunate that single phase alloys  - 38 -  could not be obtained over the complete range, of compositions i n the two systems. Bohr magneton values expected f o r MnooA^Q^O 1.23 and 1.58 per manganese atom respectively.  a  n  dM n  60 20 20 Zn  G  a  r  e  Since there are three  manganese atoms per unit c e l l t h i s would correspond to 3.69 and 4.74 Bohr magnetons per unit c e l l of Mn oAl2oC20  a  0  n  d  Mn60 20 20° Zn  G  ^he difference  between the two values ±6 of the order of 1 $ohr magneton and the difference between the valency of aluminum and zinc, which are corner atone, i s one. This would seem to suggest that the moment of the unit c e l l of t h i s type of a l l o y i s governed by the valency of the atom at the corner s i t e .  Hence  we might expect the magnetic moment to decrease l i n e a r l y as we go from Mn  60 20 20 *° 60Al20C20« Zn  c  Mn  Consider now the Bohr magneton value expected f o r Mn6QC 20 20 a  G  namely 1.43 Bohr magnetons per manganese atom or 4.29 Bohr magnetons per unit c e l l . yet  Gallium has the same number of valence electrons as aluminum  we obtain a d i f f e r e n t magnetic moment.  Ppssible explanations o f same are:  1. d i f f e r e n t interatomic distances 2. difference i n t o t a l number of electrons. Also i f valency of the cube corner atom were governing f a c t o r we would once more expect a l i n e a r decrease i n the magnetic moment as we go from Mh  60 20 20 Zn  C  t  0 Mn  60 »20C20 • c,  The difference i n interatomic distances i n above a l l o y systems does not appear to be a governing f a c t o r as f a r as magnetic moment i s concerned.  Consider f o r example the plot of the expected parameter versus the  expected Bohr mangeton value f o r Mn0QAl2oC20> ^ n 60 Zn 20 G 20a  n  d  ^60^*20^20  as i l l u s t r a t e d i n Figure 15. I f the parameter was a governing f a c t o r one would.expect a l i n e a r r e l a t i o n s h i p between the paramater and the Bohr  ~ 39 -  magneton value but such i s c e r t a i n l y not the case, -HD  Mn60Zn2QC20  1.5  A cd >  u o  2  o0  1.3  C  o -p  Mn Ga oC20  p  1.4  ,0  1.2  Mn6oAl2oC20  /  1.1  P3  1.0 .3.850  3.875  3.900  3.925  L a t t i c e Parameter A°  Figure 15  Variation of Bohr magneton value with l a t t i c e parameter  for Mn6oAl20p20» Mn6 Ga oC20s and Mn6oZn2oC20" 0  2  Perhaps a look at the Mn6oAl Zn o_ C20 system may serve t o x  2  x  de-emphasize even further the r o l e of the interatomic distance i n a f f e c t i n g the magnetic moment.  As the aluminum content i s increased from 0 t o 20  percent the magnetic moment decreases, reaching a minimum at approximately 5.5 percent, and then increases. l i n e a r l y over the same range.  The l a t t i c e parameter however decreases  A f a i r l y s i m i l a r state of a f f a i r s i s also  found i n the Mn6oGaxZn20-x 20 system as can be seen from the graphs i n G  the  results section.  The v a r i a t i o n o f the l a t t i c e parameter with the magnetic  moment as shown i n the above two systems c e r t a i n l y appears to point to the  fact that interatomic distance i s not a governing f a c t o r i n the a l l o y  systems under discussion.  - 40 -  Returning once again to the v a r i a t i o n of Bohr magneton value with atomic percent aluminum i n the Mn oAl Zn2o« ^20 system we note that x  0  x  the type of v a r i a t i o n obtained (namely a decrease and then a increase i n the Bohr magneton value) would seem t o further rule out any simple valency mechanism.  I f a simple valency mechanism were operative we would expect  a l i n e a r decrease i n the Bohr magneton value when going from M n 6 o Z n 2 o G 2 o to Mn oAl2oC20 0  4  Ev  e n  though single phase a l l o y s are not available i n  the Mn QGa Zn2o-x^20 beyond 6.63 percent gallium i t may be i n f e r r e d from 0  x  the r e s u l t s that the Bohr magneton value decreases with increasing gallium content up to 5.75 percent and then i t should increase i n some manner u n t i l i t reaches the value expected f o r M^oC^O^O  0  Once again we may conclude  that a simple valency mechanism i s not operative. Intensity plots made with X-ray goniometer at 20°C and -1B6°C f o r an a l l o y o f 2.85 atomic percent aluminum i n the Mn^QAl Zn2o_ ^20 x  x  system indicates that the o r i g i n a l facescentered cubic structure observed at room temperature at -186°C.  i s s l i g h t l y d i s t o r t e d becoming face-centered tetragonal  This i s s i m i l a r t o the t r a n s i t i o n mentioned e a r l i e r f o r an  a l l o y near the composition Mn QZn QC Q i n which case i t was also noted that 0  2  2  the t r a n s i t i o n i n structure corresponded to a maximum i n the saturation magnetization versus temperature  curve.  I t therefore seems j u s t i f i a b l e  i n assuming that, f o r a l l o y s i n the Mn£ oAl Zn2o- C o )  x  x  2  a  n  d M 60 n  G a  Z n x  20~x^20  systems i n which a maximum i n the saturation magnetization occurs, a t r a n s i t i o n i n structure occurs at a temperature  corresponding t o that at which the  maximum appears. However, the maximum i n the saturation magnetization curve i s not considered to be due t o the t r a n s i t i o n i n s t r u c t u r e .  In f a c t , i f we  - 41 -  use the concept outlined e a r l i e r f o r the Mn-Zn-C system, whereby we have two opposing sublattices having d i f f e r e n t Curie points i . e . an ordering of manganese atoms, then i t appears that the t r a n s i t i o n i n structure i s due to ordering of manganese atoms which occurs at a temperature corresponding t o the maximum i n the saturation magnetization curve. No attempt w i l l be made t o t r y and explain the unexpected type of v a r i a t i o n of Bohr magneton value with atomic percent aluminum or gallium i n the Mn6o ^x 20-x '20 A  Zn  <  o  r  ^ 60 x 20-xO20 systems. 1  Ga  Zn  Similarly  the mechanism operative i n causing maximum i n saturation magnetization curves w i l l not be discussed f u r t h e r .  We s h a l l note that the magnetic  anomaly appears to dissappear near an aluminum content of 5.5  atomic  percent i n Mn60Al Zn Q_ C o system and near a gallium content of 5.75 x  2  x  2  atomic percent i n Mn6QGa Zn20-xC20 system. x  Considering the t r a n s i t i o n  temperatures i n the a l l o y s possessing an anomaly i n saturation magnetization p l o t , i t i s found that the t r a n s i t i o n temperature decreases with increasing aluminum or gallium thus i n d i c a t i n g that i t requires a lower temperature f o r ordering of the manganese atoms to occur. I t i s f e l t that i n order to t r y and explain magnetic properties Of above systems that one would have to take i n t o account such items as t o t a l number of electrons and exchange forces between these electrons. Such a study would be rather d i f f i c u l t and i s beyond the scope of t h i s investigation.  - 42 -  VI.  1.  BIBLIOGRAPHY  F. B r a i l s f o r d , Magnetic Materials (1951) 29.  2. R.G. Butters, H.P. Myers, Philosophical Magazine, 3.  R.G. Butters, H.P. Myers, Philosophical Magazine,  4. L. Neel, Annales de Physique, (1948), 3, 137.  (1955), 46, 895. (1955), 46, 132.  

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